A kind of anti-atomic oxygen polyimide composite film and preparation method thereof

An oxygen polyimide, polyamic acid gel film technology, applied in the coating and other directions, can solve the problems of sharp physical or chemical interaction at the interface, cracking or peeling of the protective layer, low adhesion of the protective layer, etc. The effect of simple chemical forming process, maintaining mechanical properties, and controllable film thickness

Active Publication Date: 2021-08-31
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the characteristics of insoluble, infusible, and chemical corrosion resistance (except for strong alkali) of polyimide film lead to sharp interface between the protective surface layer and polyimide substrate, and it is difficult to form a stable physical or chemical interaction. The surface of polyimide film has low adhesion and is easy to peel off, or in the space environment such as cold and heat cycle, atomic oxygen erosion, particle irradiation, etc., it is very easy to cause cracking or peeling of the protective layer due to the existence of interfacial stress, and then atomic oxygen undercutting

Method used

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  • A kind of anti-atomic oxygen polyimide composite film and preparation method thereof
  • A kind of anti-atomic oxygen polyimide composite film and preparation method thereof
  • A kind of anti-atomic oxygen polyimide composite film and preparation method thereof

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preparation example Construction

[0044]Preparation of polyamic acid resin solution. Under stirring conditions, dissolve the diamine in the organic solvent, add the dianhydride monomer in batches (at least twice), and continue stirring at room temperature (15-30°C) for 3-12 hours to obtain a polyamic acid resin solution . The solid content of the obtained polyamic acid resin solution may be 10-25 wt%. Among them, the diamine can be 4,4'-diaminodiphenyl ether (4,4'-ODA), p-phenylenediamine (p-PDA), m-phenylenediamine (m-PDA), 2,2-bis [4-(4-aminophenoxy)phenyl]propane (BAPP), 3,3'-diaminodiphenyl ether (3,3'-ODA) or 1,3-bis(4-aminophenoxy ) At least one of benzene (TPER). The dianhydride can be pyromellitic dianhydride (PMDA), 2,3',3,4'-biphenyltetracarboxylic dianhydride (a-BPDA), 3,3',4,4'-biphenyltetracarboxylic acid Dianhydride (s-BPDA), 4,4'-oxydiphthalic anhydride (ODPA), 4,4'-(hexafluoroisopropylene) diphthalic anhydride (6FDA), 4,4'-(4, At least one of 4'isopropyldiphenoxy)bis(phthalic anhydride) (B...

Embodiment 1

[0062] 1) Put 80kg of dimethylacetamide solvent (DMAC) and 9.57kg of 4,4'-diaminodiphenyl ether (ODA) into the dry reaction kettle, stir until ODA is completely dissolved, then slowly add pyromellitic acid in turn Dianhydride (PMDA) 5kg, 3kg, 2kg and 0.43kg, feed intake interval 1 hour each time, continue to stir at room temperature for 8 hours, obtain the polyamic acid resin (substrate solution) that solid content is 20%;

[0063] 2) Weigh 518 grams of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in a mixed solvent consisting of 2.63 kg of dioxane and 3.95 kg of dimethylacetamide solvent (DMAC), and weigh 367 grams of Pyrellitic dianhydride (PMDA) was added into the above solution twice, and stirred at room temperature for 2 hours; continue to add 500 grams of aminobis-blocked polysiloxane (wherein, R is vinyl, T is methyl, a=10.3, b=3.2), after stirring for 1 hour, slowly add 295.4 grams of PMDA, and stir overnight at room temperature to obtain a polyamic acid / polysiloxa...

Embodiment 2

[0070] The preparation process of the preparation method of the anti-atomic oxygen polyimide film in this embodiment 2 refers to implementation 1, the difference is only: the wet coating amount of the transition layer in step 5) is about 50g / m 2 , step 6) in the coating amount of atomic oxygen protection layer is about 20g / m 2 . In the obtained anti-atomic oxygen polyimide film, the thickness of the substrate is about 30 μm, the thickness of the transition layer is about 7.5 μm, and the thickness of the anti-atomic oxygen layer is about 9 μm.

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Abstract

The invention relates to an atomic oxygen-resistant polyimide composite film and a preparation method thereof. The preparation method of the atomic oxygen-resistant polyimide film comprises: (1) coating a polyamic acid resin solution on the surface of a carrier to obtain The polyamic acid liquid film is then dried at 60-220°C for 1-20 minutes and peeled off from the carrier to obtain a polyamic acid gel film; (2) Coating polyamic acid / polyamic acid on at least one side of the polyamic acid gel film After the solution of polysiloxane block copolymer, dry at 50-100°C for 10-180 seconds to form a transition layer on at least one side of the polyamic acid gel film; (3) Continue coating on the surface of the transition layer After self-crosslinking the trapezoidal polysilsesquioxane solution, dry at 60-120°C for 10-120 seconds to obtain a multi-layer composite film; (4) The obtained multi-layer composite film is subjected to multi-stage drying treatment in a clamped state , to obtain the anti-atomic oxygen polyimide film.

Description

technical field [0001] The invention relates to an anti-atomic oxygen coating and an integrated forming method thereof, in particular to a polyimide-based anti-atomic oxygen composite film and a preparation method thereof, belonging to the field of film preparation. Background technique [0002] Polyimide (PI) has excellent performance in terms of tensile strength, thermal stability, insulation, and space radiation resistance, and is widely used in flexible thermal control materials for spacecraft and substrates for flexible solar cell arrays. However, when applied in low earth orbit, polyimide is severely eroded by atomic oxygen (AO), and the loss of mass directly leads to the rapid attenuation of the optical, thermal and mechanical properties of the material, which greatly limits the service life of the film. Therefore, improving the atomic oxygen resistance of polyimide films has always been an important research topic at home and abroad. [0003] The improvement of poly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J7/04C08J5/18C09D179/08C09D183/07C08G73/10C08G77/20C08G77/06C08L79/08
CPCC08G73/1007C08G73/106C08G73/1071C08G77/06C08G77/20C08G77/80C08J5/18C08J7/042C08J2379/08C08J2479/08C08J2483/07
Inventor 徐阳齐振一
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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